CN107369800A - A kind of composite spun fiber lithium ion battery separator and preparation method thereof - Google Patents
A kind of composite spun fiber lithium ion battery separator and preparation method thereof Download PDFInfo
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- CN107369800A CN107369800A CN201710506720.9A CN201710506720A CN107369800A CN 107369800 A CN107369800 A CN 107369800A CN 201710506720 A CN201710506720 A CN 201710506720A CN 107369800 A CN107369800 A CN 107369800A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/44—Fibrous material
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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Abstract
The invention discloses a kind of composite spun fiber lithium ion battery separator, it is prepared first by the carbon nano tube dispersion liquid after surface etching treatment and 4, the mixing of 4 ' diaminodiphenyl ethers is uniformly dispersed, after room-temperature ball-milling stir process, add pyromellitic dianhydride, with the 4 of carbon nano tube surface attachment, 4 ' diaminodiphenyl ethers react, CNT is set to be dispersed in polyamic acid solution, composite spun fiber is made through spinning technique in mixed liquor again, takes ladder-elevating temperature mode to carry out hot-imide and handle to produce afterwards.Pass through ball grinding stirring PROCESS FOR TREATMENT in the present invention, CNT after surface etching treatment is evenly dispersed in polyimide material, so that diaphragm material has higher porosity, the defects of conventional polyolefins barrier film porosity is low, ionic conductivity is poor is breached, improves the combination property of lithium ion battery.
Description
Technical field
The present invention relates to polyimide material field, and in particular to a kind of composite spun fiber lithium ion battery separator and its
Preparation method.
Background technology
As lithium ion battery is to the hair of the dynamic fields such as electric automobile, Aero-Space, energy storage, large-scale instrument instrument
Exhibition, higher requirement is proposed to the combination property of battery.The effect of barrier film determines that it must be the microporous barrier of high-insulation, film
Itself it is used for obstructing the transmission of positive and negative interpolar electronics, and its internal hole and can enough ensures that electrolyte ion advances freely, from
And realize the charge and discharge process of battery.Therefore, on the one hand, should have higher porosity inside barrier film, with ensure electrolyte from
Son passes through；On the other hand, aperture should be maintained at appropriate size, can either allow electrolyte ion by and effectively
Barrier positive and negative electrode prevents short circuit.
Anping, Cao Liyun et al. are at it《The preparation of polyimides lithium ion battery separator and its performance study》In one text,
Polyimides lithium ion battery separator is prepared using method of electrostatic spinning, the power being assembled into using polyimides spinning barrier film
Lithium ion battery shows excellent chemical property compared to conventional polyethylene diaphragm cell, in the condition of high-multiplying power discharge
Under, polyimide diaphragm still keeps 33.6% discharge rate under up to 28.8C multiplying powers.
In recent years, researcher applies to lithium-sulphur cell positive electrode as conductive network around CNT and has done deep grind
Study carefully, show fabulous discharge capacity, cycle performance and high high rate performance.But after many traditional even modifications
CNT is used for lithium-sulphur cell positive electrode as conductive network, but shows very big capacity attenuation rate.After all, this is
Because comparatively the specific surface area and pore volume of traditional CNT are not very high, many active material sulphur are caused to be unable to access aperture
Structure and it is exposed in CNT outer wall, this causes these sulphur to be easy to come off during cycle charge-discharge to diffuse to electrolyte
In, cause electrode capacity decay quickly.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of composite spun fiber lithium ion battery separator and its preparation side
Method, the porosity of polyimide-based barrier film is improved by spinning technique.
A kind of composite spun fiber lithium ion battery separator, it is prepared the CNT after surface etching treatment point first
Dispersion liquid and 4, the mixing of 4 '-diaminodiphenyl ether is uniformly dispersed, and after room-temperature ball-milling-stir process, adds pyromellitic dianhydride,
4 adhered to carbon nano tube surface, 4 '-diaminodiphenyl ether reaction, make CNT be dispersed in polyamic acid solution,
Composite spun fiber is made through spinning technique in mixed liquor again, takes ladder-elevating temperature mode to carry out hot-imide processing i.e. afterwards
.
Comprise the following steps that：
（1）The surface etching treatment of CNT：
2-6 parts by weight of carbon nanotubes is immersed in 0.5mol/L sodium hydroxide solutions, adds 0.2-0.8 part N ' N- dimethyl methyls
Acid amides and 0.1-0.4 part triton x-100s, after magnetic agitation 30-40 minutes, are transferred in polytetrafluoroethylene (PTFE) autoclave,
160-180 DEG C of reaction 8-10 hour, filter, it is neutral repeatedly to be washed with distilled water to filtrate, is dried to obtain through at surface etch
The CNT of reason；
（2）Ball milling mixing：
1., the CNT after above-mentioned surface etching treatment is added in 50-110 part N ' dinethylformamides, ultrasonic 2-3 is small
When, uniform dispersion liquid is obtained, it is standby；
2., weigh 45-60 parts 4,4 '-diaminodiphenyl ether is added in there-necked flask, first weighs 80-160 part N ' N- dimethyl methyls
Amide solvent is added in there-necked flask, reuses the raw material that 20-40 part N ' dinethylformamide solvent flush bottle walls are adhered to, and is led to
Enter N2Air displacement is carried out, stirs to raw material be completely dissolved under nitrogen protection, add above-mentioned carbon nano tube dispersion liquid, will mix
Liquid is placed in the ball grinder with agitating function and mixed, Ball-milling Time 3-10 hours, and progress interval is shut down per ball milling 10-40 minutes
Stirring, obtains 4,4 '-diaminodiphenyl ether/CNT mixed reaction solution；
（3）The preparation of polyamic acid/CNT mixing precursor liquid：
Then 48-63 part pyromellitic dianhydrides are added to step in three batches（2）In mixed reaction solution, and keep being stirred vigorously,
Every batch of interval 25-35 minute, continue to stir 3-8 hours after its all dissolving, obtain thick polyamic acid/CNT and mix
Close precursor liquid；
（4）The preparation of spinning barrier film：
Above-mentioned mixing precursor liquid is encased in syringe, is fixed on high-voltage electrostatic spinning device, is carried out with stainless steel syringe needle
Spinning, take clean smooth aluminium foil to be laid on glass plate, as the reception substrate of spinning fibre, carry out spinning, spinning finishes
Substrate is placed in 55-65 DEG C of air dry oven afterwards and dries 6-9 hours, it is standby；
（5）Imidization is handled：
By step（4）The composite spun fiber spinned is placed on quartz glass plate, is put into vacuum tube furnace, by tube furnace
Vacuum state, in N2Take ladder-elevating temperature mode to carry out hot-imide processing under atmosphere, afterwards natural cooling, obtain fibre
Tie up film, as polyimides composite nano fiber battery diaphragm.
Wherein, the step（2）The rotating speed of middle ball mill is 200-400 revs/min.
Wherein, the step（4）Middle spinning technology parameter is that spinning voltage is 18KV, flow 0.5ml/h, adjusts spinneret
The distance between head and collecting board are 20cm.
Wherein, the step（5）Middle hot-imide handling process is specific as follows：Respectively at 80 DEG C, 100 DEG C, 200 DEG C of guarantors
Temperature 1 hour, 300 DEG C of insulations carry out gradient increased temperature processing in 2 hours.
Compared with prior art, the present invention has advantages below：
（1）The present invention by the CNT after surface etching treatment and 4,4 '-diaminodiphenyl ether mixes be uniformly dispersed after, pass through
After ball milling-stirring technique processing, add pyromellitic dianhydride and polymerisation, the strand of polyamic acid high polymer occurs with diamines
The surface of nano-particle can be grafted to, CNT easy local cluster in the material is solve thed problems, such as, makes nanometer
CNT is spreaded more evenly across in polyimide material, while the CNT aperture size after etched processing is smaller,
So that diaphragm material has higher porosity, the defects of conventional polyolefins barrier film porosity is low, ionic conductivity is poor is breached,
Improve the combination property of lithium ion battery.
（2）CNT is etched with sodium hydroxide using hydrothermal high-temperature high-pressure process in the present invention, increase effectively carbon nanometer
The specific surface area and pore volume of pipe, diaphragm material is possessed excellent absorption property to active more sulphions in lithium-sulfur cell, make
Many active material sulphur can enter in pore structure, be advantageous to suppress the loss of battery polysulfide in cyclic process.
Embodiment
A kind of composite spun fiber lithium ion battery separator, it is prepared the CNT after surface etching treatment point first
Dispersion liquid and 4, the mixing of 4 '-diaminodiphenyl ether is uniformly dispersed, and after room-temperature ball-milling-stir process, adds pyromellitic dianhydride,
4 adhered to carbon nano tube surface, 4 '-diaminodiphenyl ether reaction, make CNT be dispersed in polyamic acid solution,
Composite spun fiber is made through spinning technique in mixed liquor again, takes ladder-elevating temperature mode to carry out hot-imide processing i.e. afterwards
.
Comprise the following steps that：
（1）The surface etching treatment of CNT：
5 parts by weight of carbon nanotubes are immersed in 0.5mol/L sodium hydroxide solutions, add 0.2 part of N ' dinethylformamide and
0.1 part of triton x-100, magnetic agitation are transferred in polytetrafluoroethylene (PTFE) autoclave after 30 minutes, small in 160 DEG C of reactions 8
When, filter, it is neutral repeatedly to be washed with distilled water to filtrate, is dried to obtain the CNT through surface etching treatment；
（2）Ball milling mixing：
1., the CNT after above-mentioned surface etching treatment is added in 90 parts of N ' dinethylformamides, ultrasound 3 hours, obtain
It is standby to uniform dispersion liquid；
2., weigh 58 part 4,4 '-diaminodiphenyl ether is added in there-necked flask, and it is molten first to weigh 130 parts of N ' dinethylformamides
Agent is added in there-necked flask, is reused the raw material that 30 parts of N ' dinethylformamide solvent flush bottle walls are adhered to, is passed through N2Carry out
Air is replaced, and stirs to raw material be completely dissolved under nitrogen protection, add above-mentioned carbon nano tube dispersion liquid, mixed liquor is placed in into band
Have in the ball grinder of agitating function and mix, Ball-milling Time 8 hours, shut down per ball milling 30 minutes and carry out intermittent stirring, obtain 4,4 '-
Diaminodiphenyl ether/CNT mixed reaction solution；
（3）The preparation of polyamic acid/CNT mixing precursor liquid：
Then 60 parts of pyromellitic dianhydrides are added to step in three batches（2）In mixed reaction solution, and keep being stirred vigorously, every batch
Interval 30 minutes, continue stirring 5 hours after its all dissolving, obtain thick polyamic acid/CNT mixing precursor liquid；
（4）The preparation of spinning barrier film：
Above-mentioned mixing precursor liquid is encased in syringe, is fixed on high-voltage electrostatic spinning device, is carried out with stainless steel syringe needle
Spinning, take clean smooth aluminium foil to be laid on glass plate, as the reception substrate of spinning fibre, carry out spinning, spinning finishes
Substrate is placed in 60 DEG C of air dry ovens afterwards and dried 8 hours, it is standby；
（5）Imidization is handled：
By step（4）The composite spun fiber spinned is placed on quartz glass plate, is put into vacuum tube furnace, by tube furnace
Vacuum state, in N2Take ladder-elevating temperature mode to carry out hot-imide processing under atmosphere, afterwards natural cooling, obtain fibre
Tie up film, as polyimides composite nano fiber battery diaphragm.
Wherein, the step（2）The rotating speed of middle ball mill is 400 revs/min.
Wherein, the step（4）Middle spinning technology parameter is that spinning voltage is 18KV, flow 0.5ml/h, adjusts spinneret
The distance between head and collecting board are 20cm.
Wherein, the step（5）Middle hot-imide handling process is specific as follows：Respectively at 80 DEG C, 100 DEG C, 200 DEG C of guarantors
Temperature 1 hour, 300 DEG C of insulations carry out gradient increased temperature processing in 2 hours.
Claims (5)
1. a kind of composite spun fiber lithium ion battery separator, it is characterised in that it is prepared first by after surface etching treatment
Carbon nano tube dispersion liquid and 4, the mixing of 4 '-diaminodiphenyl ether is uniformly dispersed, and after room-temperature ball-milling-stir process, adds equal
Benzene tetracarboxylic acid acid anhydride, 4 with carbon nano tube surface attachment, the reaction of 4 '-diaminodiphenyl ether, CNT is dispersed in polyamides
In amino acid solution, then composite spun fiber is made through spinning technique in mixed liquor, takes ladder-elevating temperature mode to carry out hot acyl afterwards
Imidization, which is handled, to be produced.
2. a kind of preparation method of composite spun fiber lithium ion battery separator according to claims 1, its feature exist
In comprising the following steps that：
（1）The surface etching treatment of CNT：
2-6 parts by weight of carbon nanotubes is immersed in 0.5mol/L sodium hydroxide solutions, adds 0.2-0.8 part N ' N- dimethyl methyls
Acid amides and 0.1-0.4 part triton x-100s, after magnetic agitation 30-40 minutes, are transferred in polytetrafluoroethylene (PTFE) autoclave,
160-180 DEG C of reaction 8-10 hour, filter, it is neutral repeatedly to be washed with distilled water to filtrate, is dried to obtain through at surface etch
The CNT of reason；
（2）Ball milling mixing：
1., the CNT after above-mentioned surface etching treatment is added in 50-110 part N ' dinethylformamides, ultrasonic 2-3 is small
When, uniform dispersion liquid is obtained, it is standby；
2., weigh 45-60 parts 4,4 '-diaminodiphenyl ether is added in there-necked flask, first weighs 80-160 part N ' N- dimethyl methyls
Amide solvent is added in there-necked flask, reuses the raw material that 20-40 part N ' dinethylformamide solvent flush bottle walls are adhered to, and is led to
Enter N2Air displacement is carried out, stirs to raw material be completely dissolved under nitrogen protection, add above-mentioned carbon nano tube dispersion liquid, will mix
Liquid is placed in the ball grinder with agitating function and mixed, Ball-milling Time 3-10 hours, and progress interval is shut down per ball milling 10-40 minutes
Stirring, obtains 4,4 '-diaminodiphenyl ether/CNT mixed reaction solution；
（3）The preparation of polyamic acid/CNT mixing precursor liquid：
Then 48-63 part pyromellitic dianhydrides are added to step in three batches（2）In mixed reaction solution, and keep being stirred vigorously,
Every batch of interval 25-35 minute, continue to stir 3-8 hours after its all dissolving, obtain thick polyamic acid/CNT and mix
Close precursor liquid；
（4）The preparation of spinning barrier film：
Above-mentioned mixing precursor liquid is encased in syringe, is fixed on high-voltage electrostatic spinning device, is carried out with stainless steel syringe needle
Spinning, take clean smooth aluminium foil to be laid on glass plate, as the reception substrate of spinning fibre, carry out spinning, spinning finishes
Substrate is placed in 55-65 DEG C of air dry oven afterwards and dries 6-9 hours, it is standby；
（5）Imidization is handled：
By step（4）The composite spun fiber spinned is placed on quartz glass plate, is put into vacuum tube furnace, by tube furnace
Vacuum state, in N2Take ladder-elevating temperature mode to carry out hot-imide processing under atmosphere, afterwards natural cooling, obtain fibre
Tie up film, as polyimides composite nano fiber battery diaphragm.
3. a kind of preparation method of composite spun fiber lithium ion battery separator according to claims 2, its feature exist
In the step（2）The rotating speed of middle ball mill is 200-400 revs/min.
4. a kind of preparation method of composite spun fiber lithium ion battery separator according to claims 2, its feature exist
In the step（4）Middle spinning technology parameter is that spinning voltage is 18KV, flow 0.5ml/h, adjusts spinning head and collecting board
The distance between be 20cm.
5. a kind of preparation method of composite spun fiber lithium ion battery separator according to claims 2, its feature exist
In the step（5）Middle hot-imide handling process is specific as follows：1 hour is incubated respectively at 80 DEG C, 100 DEG C, 200 DEG C,
300 DEG C of insulations carry out gradient increased temperature processing in 2 hours.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109390534A (en) * | 2018-09-10 | 2019-02-26 | 中原工学院 | A kind of nano fibrous membrane and preparation method thereof for lithium ion battery separator |
| CN110247005A (en) * | 2019-05-28 | 2019-09-17 | 浙江大学 | A kind of preparation method of the difunctional composite diaphragm for lithium-sulfur cell |
| CN110350128A (en) * | 2019-06-17 | 2019-10-18 | 浙江大学衢州研究院 | A kind of preparation method of the composite diaphragm for lithium-sulfur cell |
| CN111070722A (en) * | 2018-10-19 | 2020-04-28 | 哈尔滨工业大学 | Preparation method of lightning protection composite material based on heat insulation and insulation mechanism |
| CN111342054A (en) * | 2018-12-18 | 2020-06-26 | 现代自动车株式会社 | Positive electrode for lithium-air battery, method for preparing same, and lithium-air battery comprising same |
| CN112865239A (en) * | 2021-01-22 | 2021-05-28 | 苏州大学 | Preparation method of wireless charging device capable of being sewn on fabric and device |
| CN114044901A (en) * | 2021-12-14 | 2022-02-15 | 北京科技大学 | Polyimide material and preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109390534A (en) * | 2018-09-10 | 2019-02-26 | 中原工学院 | A kind of nano fibrous membrane and preparation method thereof for lithium ion battery separator |
| CN111070722A (en) * | 2018-10-19 | 2020-04-28 | 哈尔滨工业大学 | Preparation method of lightning protection composite material based on heat insulation and insulation mechanism |
| CN111070722B (en) * | 2018-10-19 | 2021-10-22 | 哈尔滨工业大学 | Preparation method of lightning protection composite material based on heat insulation and insulation mechanism |
| CN111342054A (en) * | 2018-12-18 | 2020-06-26 | 现代自动车株式会社 | Positive electrode for lithium-air battery, method for preparing same, and lithium-air battery comprising same |
| CN110247005A (en) * | 2019-05-28 | 2019-09-17 | 浙江大学 | A kind of preparation method of the difunctional composite diaphragm for lithium-sulfur cell |
| CN110350128A (en) * | 2019-06-17 | 2019-10-18 | 浙江大学衢州研究院 | A kind of preparation method of the composite diaphragm for lithium-sulfur cell |
| CN110350128B (en) * | 2019-06-17 | 2021-11-30 | 浙江大学衢州研究院 | Preparation method of composite diaphragm for lithium-sulfur battery |
| CN112865239A (en) * | 2021-01-22 | 2021-05-28 | 苏州大学 | Preparation method of wireless charging device capable of being sewn on fabric and device |
| CN114044901A (en) * | 2021-12-14 | 2022-02-15 | 北京科技大学 | Polyimide material and preparation method and application thereof |
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Application publication date: 20171121 |